CN103102925B - Hydrogenation method for producing high quality low freezing point motor fuel from biological oil - Google Patents
Hydrogenation method for producing high quality low freezing point motor fuel from biological oil Download PDFInfo
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- CN103102925B CN103102925B CN201110353852.5A CN201110353852A CN103102925B CN 103102925 B CN103102925 B CN 103102925B CN 201110353852 A CN201110353852 A CN 201110353852A CN 103102925 B CN103102925 B CN 103102925B
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- Y02P30/00—Technologies relating to oil refining and petrochemical industry
- Y02P30/20—Technologies relating to oil refining and petrochemical industry using bio-feedstock
Abstract
The present invention relates to a hydrogenation method for producing a high quality low freezing point motor fuel from a biological oil. The method is characterized in that a biological oil is adopted as a raw material oil; under a hydrogenation operation condition, the raw material oil and hydrogen gas pass through a first stage hydrogenation reaction zone containing at least two hydrogenation reactors, wherein the raw material oil and the hydrogen gas sequentially pass through a low temperature operation reactor and a high temperature operation reactor; hydrogen-rich gas separated from the stream generated from hydrogenation is recycled, and the separated liquid enters a second stage hydrogenation modification reaction zone; sub-hydrogen gas separated from the stream generated from hydrogenation modification is recycled, and the separated liquid product is subjected to fractionation to obtain naphtha and a low freezing point diesel oil; and under a reaction state, active components of the hydrogenation catalysts used at the first stage and the second stage are sulfurization state Pt and/or Pd. Compared to the method in the prior art, the method of the present invention has the following advantages that: storage stability can be effectively improved when the biological oil is adopted as a fuel oil, and hydrogenation device stability can be effectively prolonged.
Description
Technical field
The present invention relates to a kind of method of hydrotreating, particularly a kind of is stock oil with bio-oil, the method for hydrotreating of direct production high-grade low-freezing point automotive fuel.
Background technology
The energy in current global range is mainly derived from fossil energy, and its PetroChina Company Limited. is the main source of automotive fuel.Oil belongs to Nonrenewable energy resources, not only resource is day by day exhausted, and heaviness and in poor quality aggravation, and world economy sustainable development, environmental regulation increasingly stringent need to produce a large amount of light clean fuel, these increase new oil substitutes while all requiring to improve existing oil Refining Technologies, produce satisfactory product with minimum cost.
Bio-oil, as renewable resources, obtains the extensive attention in the world, and each research unit and enterprise are all making great efforts to carry out its research as clean energy.The method production biofuel (being generally fatty acid methyl ester) utilizing transesterify has been proven technique, but because fatty acid methyl ester oxygen level is high, although many countries and regions have put into effect the standard of biofuel successively, and are not suitable for all oil engines.Bio-oil produces automotive fuel by the method for hydrogenation, and all remove by oxygen or partly remove the product produced and meet automotive fuel standard, this method directly can meet the requirement of existing market.
Existing animal-plant oil hydrogenation method produces the processing technology of automotive fuel, US20060186020, EP1693432, CN101321847A, CN200710012090.6, CN200680045053.9, CN200710065393.4, CN200780035038.0, CN200710012208.5, CN200780028314.0 and CN101029245A etc. disclose vegetables oil hydroconversion process, adopt coker naphtha, diesel oil distillate (straight-run diesel oil, LCO and coker gas oil), the petroleum hydrocarbon cuts such as wax oil cut and bio-oil are mixed into hydrogenation catalyst bed, produce diesel product or preparing ethylene by steam cracking raw material etc.US5705722 discloses the diesel oil blending component producing diesel oil distillate scope containing the vegetables oil such as unsaturated fatty acids, fat and animal oil mixing back end hydrogenation.
EP1741767 and EP1741768 discloses a kind of method of producing diesel oil distillate with animal-plant oil, be mainly animal-plant oil first through hydrotreatment, then by isomerization catalyst bed layer, obtain low freezing point diesel fuel component, but owing to generating water in hydroprocessing processes, cause very adverse influence to isomerization catalyst, device can not long-period stable operation.
Comprise in the bio-oil hydrogenation process of aforesaid method, one of subject matter run into is the less stable of catalyzer, and running period shortens, and needs more catalyst changeout of often stopping work.Particularly independent with bio-oil be raw material or bio-oil blending ratio higher time, the running period of hydrogenation catalyst is more subject to obvious impact, cannot meet the requirement of industrial application.
In prior art, bio-oil hydrogenation produces the method for automotive fuel, the petroleum fractions hybrid process of general needs and larger proportion, otherwise can not running period be ensured, or directly by hydrofining-catalyst for hydro-upgrading bed, the component poor stability of cracking catalyst activity.The present invention is by optimizing the grating technology and operational condition that use catalyzer, one stage hydrofining (operational condition of optimization and the hydrogenation catalyst of composition grating), secondary hydrogenation upgrading, it can be directly raw material production high-grade low-freezing point automotive fuel with bio-oil, solving bio-oil hydrogenation unit can not the problem of long period steady running, significantly can reduce the condensation point of diesel oil distillate simultaneously.
Summary of the invention
For the deficiencies in the prior art, the invention provides the method for hydrotreating that a kind of bio-oil produces high-grade low-freezing point automotive fuel, can be separately stock oil with animal-plant oil, the method of direct production automotive fuel under the condition of hydrogenation, can the high-quality diesel oil blending product of direct production, the situation that diesel product can not be occurred biofuel that conventional animal-plant oil obtains is gone mouldy, can ensure that hydrogenation catalyst has longer running period simultaneously, be suitable for industrial application.
The method of hydrotreating that bio-oil of the present invention produces high-grade low-freezing point automotive fuel comprises following content:
A one or more in () bio-oil are stock oil;
B () is under Hydroprocessing conditions, stock oil and hydrogen pass through the first paragraph reaction zone of at least two hydrogenators, hydrogenation catalyst is loaded in hydrogenator, stock oil and hydrogen are first by the hydrogenator of cold operation, then by the hydrogenator of high-temperature operation, under response behaviour, the active ingredient of hydrogenation catalyst is Pt and/or Pd of reduction-state;
C () first paragraph reaction zone hydrogenation effluent is separated into gas phase and liquid phase, gas-phase dehydration process Posterior circle uses, the second segment reaction zone using catalyst for hydro-upgrading is entered after liquid phase mixes with circulation gas, under response behaviour, the active metal component of catalyst for hydro-upgrading is Pt and/or Pd of reduction-state;
D the gas phase of () second segment reaction zone reaction effluent recycles, liquid phase fractionation in separation column of second segment reaction zone reaction effluent obtains petroleum naphtha and low freezing point diesel fuel.
In the inventive method step (a), the bio-oil used can comprise vegetables oil or animal grease, vegetables oil comprises one or more in soybean oil, peanut oil, Viscotrol C, rapeseed oil, Semen Maydis oil, sweet oil, plam oil, Oleum Cocois, tung oil, oleum lini, sesame oil, Oleum Gossypii semen, sunflower seed oil and rice bran wet goods, and animal grease comprises one or more in butter, lard, sheep oil and fish oil etc.
In the inventive method step (b), the Hydroprocessing conditions of the hydrotreating reactor of cold operation is generally reaction pressure 3.0MPa ~ 20.0MPa, and hydrogen to oil volume ratio is 200:1 ~ 3000:1, and volume space velocity is 0.3h
-1~ 6.0h
-1, average reaction temperature 120 DEG C ~ 280 DEG C; The operational condition of the hydrotreating reactor of high-temperature operation is reaction pressure 3.0MPa ~ 20.0MPa, hydrogen to oil volume ratio 200:1 ~ 3000:1, volume space velocity 0.3h
-1~ 6.0h
-1, average reaction temperature is higher than the hydrotreating reactor of cold operation 50 DEG C ~ 300 DEG C, preferably high 80 ~ 220 DEG C.Process furnace or interchanger are set between the hydrotreating reactor of cold operation and the hydrotreating reactor of high-temperature operation, to adjust the temperature of reaction of the hydrotreating reactor of high-temperature operation.
Reaction mass is first by the hydrogenator of cold operation, and the active ingredient of the hydrogenation catalyst of use is in the element quality of precious metals pt and/or Pd, and the content of noble metal hydrogenation active ingredient is 0.01% ~ 0.50%.Reaction mass continues through the hydrogenator of high-temperature operation, and the active ingredient of the hydrogenation catalyst used in the hydrogenator of high-temperature operation is in the element of precious metals pt and/or Pd, and the content of noble metal hydrogenation active ingredient is 0.10% ~ 3.50%.In the hydrogenator of preferred high-temperature operation, the active component content of catalyzer is higher than the catalyzer in cold operation hydrogenator, preferably high 0.1 ~ 3 percentage point (in element quality).Reactor generally can arrange 2 ~ 5, is preferably 2.A kind of catalyzer can be loaded in each hydrogenator, also can load multiple catalysts.
The carrier of hydrogenation catalyst is generally aluminum oxide, amorphous silicon aluminium, silicon oxide, titanium oxide etc., can contain other auxiliary agent, as P, Si, B, Ti, Zr etc. simultaneously.Can commercial catalyst be adopted, also can by the existing method preparation in this area.Noble metal catalyst such as Fushun Petrochemical Research Institute (FRIPP) develops HDO-18 catalyzer, also can by described method preparations such as CN00123141.3.
In the inventive method step (b), catalyzer uses hydrogen 200 DEG C ~ 500 DEG C temperature before use, reduces under preferably 220 DEG C ~ 450 DEG C conditions.Whenever forbid in system, inject sulfur-bearing, nitrogenous medium, avoid poisoning of catalyst.
In the inventive method step (c), the Hydroprocessing conditions of second segment reaction zone is generally reaction pressure 3.0MPa ~ 20.0MPa, usually (pressure rating that identical finger herein identical identical with first paragraph reaction zone, due to the Pressure Drop of Flow of Goods and Materials, second segment reaction zone reaction pressure can a little less than first paragraph reaction zone), hydrogen to oil volume ratio is 200:1 ~ 3000:1, and volume space velocity is 0.3h
-1~ 6.0h
-1, average reaction temperature 180 DEG C ~ 465 DEG C; Preferred operational condition is hydrogen to oil volume ratio 300:1 ~ 2500:1, volume space velocity 0.4h
-1~ 4.0h
-1, average reaction temperature 200 DEG C ~ 445 DEG C.
In the inventive method step (c), the catalyst for hydro-upgrading of second reaction zone has isomery function, as containing components such as beta-molecular sieve, SAPO-11 molecular sieve, SAPO-41, NU-10 molecular sieve or ZSM-22 molecular sieves.Catalyst for hydro-upgrading is in the element of precious metals pt and/or Pd, and the content of noble metal hydrogenation active ingredient is 0.01% ~ 0.50%.The massfraction of catalyst for hydro-upgrading Middle molecule sieve is generally 5% ~ 40%.Other component in catalyst for hydro-upgrading is generally the porous refractory oxide such as aluminum oxide, silicon oxide, amorphous aluminum silicide.
In the inventive method, catalyzer uses hydrogen 200 DEG C ~ 500 DEG C temperature before use, reduces under preferably 220 DEG C ~ 450 DEG C conditions.Whenever forbid in system, inject sulfur-bearing, nitrogenous medium, avoid poisoning of catalyst.
Accompanying drawing explanation
Fig. 1 is the method for hydrotreating principle flow chart of bio-oil production high-quality automotive fuel of the present invention.
Embodiment
Method of the present invention is specific as follows: with the mixing oil of one or more in bio-oil for stock oil, under Hydroprocessing conditions, stock oil and hydrogen pass through low temperature and the high temperature hydrogenation reactor of loading catalyst, the hydrogenated oil obtained is separated in high-pressure separator (abbreviation high score) gas circulation obtained and uses, also system can be gone out, the liquid fractionation obtained and hydrogen are mixed into the second segment reaction zone comprising and have isomery performance catalyst for hydro-upgrading, obtain hydro-upgrading logistics and be separated the gas circulation use obtained in high-pressure separator (abbreviation high score), the liquid fractionation obtained obtains following products: gas, petroleum naphtha, one or more in low freezing point diesel fuel, if improve the character of diesel product further or extend the cycle of operation, also can consider that a part of diesel oil and unconverted oil loop back reactive system.The bio-oil that embodiment uses is commercially available prod, uses front filtering solid impurity.
Particular case of the present invention is further illustrated below by embodiment.
The main composition of table 1 hydrogenation catalyst and character.
Catalyzer | Catalyzer 1 | Catalyzer 2 | Catalyzer 3 | Modifying catalyst |
Catalyzer forms | ? | ? | ? | ? |
Pt,wt% | 0.4 | 1.2 | 0.05 | 1.0 |
Pd,wt% | 0.1 | ? | 0.1 | 0.1 |
Beta-molecular sieve, wt% | ? | ? | ? | 15.0 |
Alumina supporter, wt% | Surplus | Surplus | Surplus | Surplus |
The main character of catalyzer | ? | ? | ? | ? |
Specific surface, m 2/g | >160 | >160 | >160 | >160 |
Pore volume, ml/g | 0.33 | 0.32 | 0.35 | 0.34 |
Table 2 embodiment processing condition and test-results.
Processing condition | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 |
Stock oil | Soybean oil | Rapeseed oil | Tung oil | Oleum Gossypii semen |
First paragraph reaction zone operational condition | ? | ? | ? | ? |
Cold operation reactor | ? | ? | ? | ? |
Catalyzer | Catalyzer 3 | Catalyzer 3/ catalyzer 1 | Catalyzer 3/ catalyzer 1 | Catalyzer 3 |
Catalyst volume ratio | 100 | 20:80 | 50:50 | 100 |
Reaction pressure, MPa | 17.0 | 5.0 | 10.0 | 12.0 |
Entrance hydrogen to oil volume ratio | 2000:1 | 300:1 | 1000:1 | 800:1 |
Volume space velocity, h -1 | 2.0 | 1.5 | 0.8 | 0.4 |
Average reaction temperature, DEG C | 150 | 190 | 130 | 100 |
High-temperature operation reactor | ? | ? | ? | ? |
Catalyzer | Catalyzer 1 | Catalyzer 1 | Catalyzer 2 | Catalyzer 2 |
Reaction pressure, MPa | 17.0 | 5.0 | 10.0 | 12.0 |
Entrance hydrogen to oil volume ratio | 2000:1 | 300:1 | 1000:1 | 1000:1 |
Volume space velocity, h -1 | 1.0 | 1.8 | 0.5 | 2.5 |
Average reaction temperature, DEG C | 360 | 320 | 340 | 380 |
Per pass conversion, quality % | 90 | 75 | 85 | 100 |
Second segment reaction zone operational condition | ? | ? | ? | ? |
Catalyzer | Modifying catalyst | Modifying catalyst | Modifying catalyst | Modifying catalyst |
Reaction pressure, MPa | 17.0 | 5.0 | 10.0 | 12.0 |
Entrance hydrogen to oil volume ratio | 1500 | 500 | 800 | 1000 |
Volume space velocity, h -1 | 2.0 | 4.5 | 1.5 | 3.5 |
Average reaction temperature, DEG C | 320 | 370 | 310 | 290 |
Diesel product | ? | ? | ? | ? |
Density, g/cm 3 | 0.781 | 0.779 | 0.783 | 0.784 |
Sulphur content, μ g/g | <5 | <5 | <5 | <5 |
Condensation point, DEG C | -20 | -35 | -15 | -10 |
Cetane value | >80 | >80 | >80 | >80 |
Table 3 embodiment processing condition and test-results.
Processing condition | Embodiment 5 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
Stock oil | Oleum Gossypii semen | Oleum Gossypii semen | Oleum Gossypii semen | Oleum Gossypii semen |
Cold operation reactor | ? | ? | ? | ? |
Catalyzer | Catalyzer 3 | ? | ? | ? |
Reaction pressure, MPa | 10.0 | ? | ? | ? |
Entrance hydrogen to oil volume ratio | 2000:1 | ? | ? | ? |
Volume space velocity, h -1 | 2.5 | ? | ? | ? |
Average reaction temperature, DEG C | 180 | ? | ? | ? |
High-temperature operation reactor | ? | ? | ? | ? |
Catalyzer | Catalyzer 2 | Catalyzer 2/ modifying catalyst | Catalyzer 2/ modifying catalyst | Catalyzer 2/ modifying catalyst |
Reaction pressure, MPa | 10.0 | 10.0 | 10.0 | 10.0 |
Entrance hydrogen to oil volume ratio | 1000:1 | 1000:1 | 1000:1 | 1000:1 |
Volume space velocity, h -1 | 0.8 | 0.5 | 0.5 | 0.5 |
Average reaction temperature, DEG C | 310 | 310 | 310 | 320 |
Two step process condition | ? | — | — | — |
Catalyzer | Modifying catalyst | ? | ? | ? |
Reaction pressure, MPa | 10.0 | ? | ? | ? |
Entrance hydrogen to oil volume ratio | 1000:1 | ? | ? | ? |
Cumulative volume air speed, h -1 | 2.8 | ? | ? | ? |
Average reaction temperature, DEG C | 330 | ? | ? | ? |
Runtime, h | 1000 | 200 | 400 | 600 |
Diesel product | ? | ? | ? | ? |
Density, g/cm 3 | 0.785 | 0.786 | 0.809 | 0.862 |
Condensation point, DEG C | -20 | -19 | -5 | 12 |
Sulphur content, μ g/g | <5 | <5 | <5 | <5 |
Cetane value | >80 | >80 | 78 | 70 |
Comparative example catalyzer 2 consumption is identical with the total consumption of embodiment 5 catalyzer 2 and catalyzer 3, and comparative example modifying catalyst consumption is identical with embodiment 5 modifying catalyst consumption.As can be seen from embodiment, bio-oil can direct production high-grade low-freezing point diesel product by the method for hydrotreating of this technology, or fine-quality diesel oil blending component, and can long-time steady operation.
Claims (8)
1. bio-oil produces a method of hydrotreating for high-grade low-freezing point automotive fuel, it is characterized in that comprising following content:
A one or more in () bio-oil are stock oil;
B () is under Hydroprocessing conditions, stock oil and hydrogen pass through the first paragraph reaction zone of at least two hydrogenators, hydrogenation catalyst is loaded in hydrogenator, stock oil and hydrogen are first by the hydrogenator of cold operation, then by the hydrogenator of high-temperature operation, under response behaviour, the active ingredient of hydrogenation catalyst is Pt and/or Pd of reduction-state, in the hydrogenator of the cold operation that first reaction mass passes through, the active ingredient of the hydrogenation catalyst used is in the element quality of precious metals pt and/or Pd, the content of noble metal hydrogenation active ingredient is 0.01% ~ 0.50%, reaction mass continues through the hydrogenator of high-temperature operation, the active ingredient of the hydrogenation catalyst used in the hydrogenator of high-temperature operation is in the element of precious metals pt and/or Pd, the content of noble metal hydrogenation active ingredient is 0.10% ~ 3.50%, in the hydrogenator of high-temperature operation, the active component content of catalyzer is in element quality, higher than the catalyzer in cold operation hydrogenator 0.1 ~ 3 percentage point,
C () first paragraph reaction zone hydrogenation effluent is separated into gas phase and liquid phase, gas-phase dehydration process Posterior circle uses, the second segment reaction zone using catalyst for hydro-upgrading is entered after liquid phase mixes with circulation gas, under response behaviour, the active metal component of catalyst for hydro-upgrading is Pt and/or Pd of reduction-state;
D the gas phase of () second segment reaction zone reaction effluent recycles, liquid phase fractionation in separation column of second segment reaction zone reaction effluent obtains petroleum naphtha and low freezing point diesel fuel.
2. in accordance with the method for claim 1, it is characterized in that: in step (a), the bio-oil of use comprises vegetables oil or animal grease.
3. in accordance with the method for claim 1, it is characterized in that: in step (b), the reaction pressure 3.0MPa ~ 20.0MPa of the hydrotreating reactor of cold operation, hydrogen to oil volume ratio is 200:1 ~ 3000:1, and volume space velocity is 0.3h
-1~ 6.0h
-1, average reaction temperature 120 DEG C ~ 280 DEG C; The operational condition of the hydrotreating reactor of high-temperature operation is reaction pressure 3.0MPa ~ 20.0MPa, hydrogen to oil volume ratio 200:1 ~ 3000:1, volume space velocity 0.3h
-1~ 6.0h
-1, average reaction temperature is higher than the hydrotreating reactor of cold operation 50 DEG C ~ 300 DEG C.
4. according to the method described in claim 1 or 3, it is characterized in that: in step (b), the average reaction temperature of the hydrotreating reactor of high-temperature operation is higher than the hydrotreating reactor of cold operation 80 ~ 220 DEG C.
5. according to the method described in claim 1 or 3, it is characterized in that: the first paragraph reaction zone in step (b) arranges 2 ~ 5 reactors.
6. in accordance with the method for claim 1, it is characterized in that: in step (c), the reaction pressure of second segment reaction zone is 3.0MPa ~ 20.0MPa, and hydrogen to oil volume ratio is 200:1 ~ 3000:1, and volume space velocity is 0.3h
-1~ 6.0h
-1, average reaction temperature 180 DEG C ~ 465 DEG C.
7. in accordance with the method for claim 1, it is characterized in that: in step (c), the hydrogen to oil volume ratio of second segment reaction zone is 300:1 ~ 2500:1, and volume space velocity is 0.4h
-1~ 4.0h
-1, average reaction temperature is 200 DEG C ~ 445 DEG C.
8. according to the method described in claim 1 or 6, it is characterized in that: in step (c), the catalyst for hydro-upgrading of second segment reaction zone has isomery function, catalyst for hydro-upgrading contains beta-molecular sieve, SAPO-11 molecular sieve, SAPO-41, NU-10 molecular sieve or ZSM-22 molecular sieve, catalyst for hydro-upgrading is in the element quality of precious metals pt and/or Pd, and the content of noble metal hydrogenation active ingredient is 0.01% ~ 0.50%.
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CN101321847A (en) * | 2005-11-30 | 2008-12-10 | 新日本石油株式会社 | Hydrorefining process and hydrorefined oil |
CN101617029A (en) * | 2007-02-20 | 2009-12-30 | 国际壳牌研究有限公司 | Produce the method for paraffinic hydrocarbons |
CN102041023A (en) * | 2009-10-16 | 2011-05-04 | 中国石油化工股份有限公司 | Method for improving residual oil hydrogenation by blending biological grease |
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BRPI0500591A (en) * | 2005-02-18 | 2006-10-03 | Petroleo Brasileiro Sa | process for hydroconversion of vegetable oils |
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CN101321847A (en) * | 2005-11-30 | 2008-12-10 | 新日本石油株式会社 | Hydrorefining process and hydrorefined oil |
CN101617029A (en) * | 2007-02-20 | 2009-12-30 | 国际壳牌研究有限公司 | Produce the method for paraffinic hydrocarbons |
CN102041023A (en) * | 2009-10-16 | 2011-05-04 | 中国石油化工股份有限公司 | Method for improving residual oil hydrogenation by blending biological grease |
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